反应详情

130 mg of 2-(4-chloro-3-difluoromethyl-2-pyridyl)-2-cyclopropyl-1-methoxyethene (XI) was dissolved in 10 ml of THF, which was added 3 ml of dilute sulfuric acid and concentrated at 50° C. under reduced pressure. The resulting mixture was poured into water and neutralized with saturated sodium bicarbonate solution, and thereafter, extracted with chloroform. The resulting organic layer was washed with saturated salt water, and thereafter, dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent; hexane:ethyl acetate=4:1) to obtain 70 mg of 2-(4-chloro-3-difluoromethyl-2-pyridyl)-2-cyclopropylethanal (XII).

1. concentrationconcentrated at 50° C. under reduced pressure
2. additionThe resulting mixture was poured into water and neutralized with saturated sodium bicarbonate solution
3. extractionextracted with chloroform
4. washThe resulting organic layer was washed with saturated salt water
5. dry with materialdried over anhydrous sodium sulfate
6. distillationthe solvent was distilled off under reduced pressure
7. customThe resulting residue was purified by silica gel column chromatography (eluent; hexane:ethyl acetate=4:1)